Separation of copolymers by adsorption liquid chromatography

Binary random copolymers of styrene with butadiene, methyl methacrylate, and t-butyl methacrylate, and styrene-methyl methacrylate-acrylonitrile random terpolymers were separated by adsorption chromatography. The HPLC conditions required for the sample to adsorb to the stationary phase are discussed. Sequence length as well as composition affected the elution volume of block and graft copolymers of styrene and butadiene. A mixture of terpolymers having different composition was separated to each component by cross-fractionation using two types of adsorption chromatography.     

Separation of iodine species by adsorption chromatography

Based on the different properties of iodide and iodate species in somesorption materials a new chromatographic method was developed to study thespeciation of iodine in a mangrove system. Two sorption materials, aluminaand silica, were investigated and several distribution coefficients for iodideand iodate were determined at different concentrations of NaOH, NaNO₃ and NaHCO₃ solutions. The best separation results wereobtained percolating sea water samples, containing iodine species, througha glass column filled with alumina. The iodide passed through the column afterwashing the column with 0.1M sodium nitrate solution, and the iodate was elutedwith a 0.5M sodium bicarbonate solution.     

Separation of inorganic anions by unsuppresed ion chromatography

The elution behaviour of 11 inorganic anions is investigated by unsuppressed ion chromatography with PRP-X100 a macroporous poly(styrene-divinylbenzene) strong-base anion-exchanger. Weak acids (cyanide and sulfide) can be separated and detected at pH 9 with sodium p-hydroxybenzoate as the eluent.     

Separation of enantiomers by gas chromatography

The separation of enantiomers by gas chromatography is performed on chiral stationary phases (CSPs) via hydrogen bonding, coordination and inclusion. Thus, typical chiral selectors are amino acid derivatives, terpene-derived metal coordination compounds and modified cyclodextrins. In Chirasil-type stationary phases the chiral selector is anchored to a polysiloxane backbone improving gas chromatographic performance. The present review article describes the state-of-the-art, scope and limitations, applications and mechanistic considerations at the advent of the millennium incorporating 16 figures and 168 references.     

Determination of adsorption by fluorescence in gas chromatography

PMBF₂, a pyrromethene pigment, can be used in gas chromatography. Because of its fluorescence, adsorption sites on glass columns and connections can be traced in situ. The compound can be employed to check the inertness of glass surfaces after deactivation procedures. Some applications are described.     

Separation of capsaicin from capsaicinoids by macroporous resin adsorption chromatography

The aim of present study is to develop an efficient and low‐cost method for capsaicin production isolated from capsaicinoids by macroporous resin adsorption chromatography. HZ816 resin has shown the best adsorption and desorption capacities for capsaicin among other resins. To optimize the operating parameters for separation, initial concentration, diameter‐to‐height ratio, mobile phase ratio, and crystallization method were investigated. When capsaicinoids solution (5 g/L) was loaded onto the column (diameter‐to‐height ratio = 1:12) with ethanol/1% w/w NaOH (4:6, v/v) as the mobile phase, capsaicin was purified most effectively. By using acid neutralization as the crystallization method, the purity of capsaicin improved from 90.3 to 99.5% with 82.3% yield. In conclusion, this study provides a simple and low‐cost method for the industrial‐scale production of high‐purity capsaicin.     

Separation and determination of inorganic anions by means of ion-pair chromatography

Bromide, iodide, bromate, iodate, thiocyanate, nitrite and nitrate can be separated by means of ion-pair chromatography on a reversed-phase column (LiChrosorb RP2), using the tricaprylylmethylammonium ion (Aliquat-336) as counter ion in an acetonitrile-water mobile phase. The elution is monitored with an ultraviolet detector at 205 and 226 nm. The detection limits are in the low nanogram range.     

Separation of short-chain branched polyolefins by high-temperature gradient adsorption liquid chromatography

A new separation principle was recently introduced into the analytical characterization of polyolefins by researchers from the German Institute for Polymers in Darmstadt. It was demonstrated that polyolefins can be selectively separated via high-performance liquid chromatography on the basis of their adsorption/desorption behaviours at temperatures as high as 160 °C. A Hypercarb? column packed with porous graphite gave the best results. The mobile phase consisted of a mixture of 1-decanol and 1,2,4-trichlorobenzene. In this work, the same chromatographic system is applied to the separation of ethylene/alkene and ethylene/norbornene copolymers. It was found that the elution volumes of the samples correlate linearly with the average chemical composition of samples. The elution volume is indirectly proportional to the concentration of branches in the ethylene/alkene copolymer. Branching shortens the length of continuous methylene sequences of the polymer backbone, thus decreasing the probability of orientation of a methylene sequence in a flat conformation on the graphite surface, which enables the most intensive van der Waals interactions between the methylene backbone and the carbon surface. An opposite trend in the elution order has been found for ethylene/norbornene copolymers. The elution volume of the ethylene/norbornene copolymers increased with the concentration of norbornene. It indicates pronounced attractive interactions between graphite and the cyclic comonomer.     

Separation of inorganic anions by reversed-phase ion-pair chromatography with direct UV detection

In this paper, a separation method of the inorganic anions including I^–, NO ₂ ^– , NO ₃ ^– , IO ₃ ^– and SCN^– on the reversed-phase ion-pair chromatography with direct UV detection has been developed, and the limits of detection of these inorganic anions were determined. The effects of the organic modifier volume fraction and concentration of the ion-pair reagent on the retention of inorganic anions were discussed.     

Determination of the solubility of inorganic salts by headspace gas chromatography

This work reports a novel method for determination of salt solubility using headspace gas chromatography. A very small amount of volatile compound (such as methanol) is added in the studied solution. Due to the molecular interaction in the solution, the vapor-liquid equilibrium (VLE) partitioning coefficient of the volatile species will change with different salt contents in the solution. Therefore, the concentration of volatile species in the vapor phase is proportional to the salt concentration in the liquid phase, which can be easily determined by headspace gas chromatography. Until the salt concentration in the solution is saturated, the concentration of volatile compound in the vapor phase will continue to increase further and a breakpoint will appear on the VLE curve. The solubility of the salts can be determined by the identification of the breakpoint. It was found that the measured solubility of sodium carbonate and sodium sulfate in aqueous solutions is slightly higher (about 6-7%) than those reported in the literature method. The present method can be easily applied to industrial solution systems.     

Separation of phenols, alcohols, and alkylbenzenes by gas chromatography on adsorption layers of copper and nickel alizarinates

The separation of mixtures of phenols, alcohols, and alkylbenzenes by gas chromatography on adsorption layers of nickel and copper alizarinates was investigated. The thermodynamic parameters were calculated. It was shown that the sorbates differ in strength of interaction with the copper and nickel ions in their alizarin complexes.     

How to count strong adsorption sites by gas chromatography?

Summary A simple gas chromatographic method is presented for the determination of the quantity of the strongest adsorption sites on an adsorbent's surface. The method consists of the blockage of the sites with quasi-irreversibly adsorbed, known amount of a strongly interacting compound and subsequent measuring of the retention of a hydrocarbon during the presence of the blocking compound in the column. Heterogeneity of chromatographic grade silicas is investigated with this method.